Method of and apparatus for liquefying chlorine gas



May 11,1926. 1,584,376

. w. M. JEWELL METHOD OF AND APPARATUS FOR LIQUEFYING CHLORINE As W zmwmm 12% 2mm v 4 c .7 7 W? a? w 9 Patented May 11, 1926.

UNITED STATES 1,584,376 PATENT OFFICE.

WIIJI JxAIVIM JEWELL, CHICAGO, ILLINOIS, ASSIGNOR TO. CfiLORINE PRODUCTS COMPANY, OF CHICAGO, ILLINOIS," A CORPORATION OF ILLINOIS.

' METHOD or AND APPARATUS FOR rQUn-rYmacrr oamE one,

'Original' application filed May 12, 1919, Serial No. 296,460. DividedandJthis' apfllic ationlfiled February 11, 1921, Serial No. $44,181.

l\/Iy'- invention relates generally to the charging into shipping containers, of, condensed gas and, more particularly, chlorine gas; and my primary objects are to provide improvements in: the methods and apparatuses heretofore used to the end that the operations may, be simplified, rendered more economical and the filling of the containers quickly effected and without danger of diluting the condensed gas in the condenser, my present invention having been divided out of my application for United States Letters Patent, Serial No. 296,460, filed May 12, 1919, patented Sept. 2, 1924, No. 1,507,289. I have chosen to illustrate my invention, by way of example, in the accompanying 1 drawing, in connection with the other details of the System disclosed in my said pending application, wherein the system referred to is shown generally matically. The accompanying drawing shows by a View, in the nature of a diagram, apparatus embodying my. invention.

In the particular apparatus shown a pipe,

diagramrepresented at 3, leads from the apparatus wherein the chlorine gas is produced, as, for example, from an electrolytic cell or cells (not shown) and which operate to produce electrolytic chlorine gas which commonly contains some non-condensable gas, this pipe connecting with the upper end of a coil 4 of a cooling apparatus 5, this coil being con; tained in a chamber 6 through which av coolin medium, as, for example, water, is circu ated,'the water entering the bottom of the tank 5through the pipe 7 and discharging therefrom at itsv top through the pipe 8. The lower end of the coil 4 connects with a trap 9 in the form of a U-pipe communicating at its lowest portion with a pipe 10 through which condensable matter removed from the chlorine gas in the coil 1, is withdrawn through the outlet pipe 11. The trap '9 connects with a'pipe 12 which opens into the bottom of a. preliminary drying tower 13 which may be of any suitable construction, the same being shown as of the loose-packing type, as represented at 14;, whereby the gas flowing into the drying tower is caused to pass in a zigzag course to the upper portion thereof from which it passes through a pipe 15 which connects with the lower end of another drying tower 16 which may be of the same generalconstruction as :described ,for the tower 13, the gaspassing iipwardly through the tower 16 and passing therefrom through a pipe 17 which connects with a coil 18. The coil 18 as shown is jacketed by the coil 19 having an inlet pipe 20 and an outlet pipe 21, this part ofthe apparatus being so constructed that chlorine gas with acid therein, as hereinafter explained, will ,pass through the coil 19 in'a direction contraryto the flow of gas through the coil 18. The end of the coil 18 opposite thatconnected with thepipe 17 is provided with a valve 22 and connects with the inlet open-i ing of'the' compressor represented at 23, a pipe 24 communicating with the outlet open shown) is lubricated by means of comparatively dry sulphuric acid, the acid by pref- .crence being at least of 1.84 specific gravity at 66 Baum 95% pure, and to accomplish this, the acid may be supplied to the interior of the crank-case 25 from which it becomes supplied to the piston for lubricating'the latter inits movements in the cylinder, by

.the action'of the connecting rod and its con nection with the crank shaft of the engine operating as a splash feed. In the particular apparatus shown, the sulphuric acid is suppliedto the crankcase 25 through a pipe 28, valved as indicated at 29, and connected with the lower end of a tank shown as supported at 31 andcommunicating by a pipe 32, valved at 33, with a sup-. ply of sulphuric acid. The upper end of the tank 30 connects by a pipe 34 with the pipe 20, the pipe 34: adjacent the tank 30 having a branch 35 provided with aventvalve 36 which is opened to permit the gas to ing in the cylinder of the compressor for\ prcssurein the chamber 30 to vent therefrom during the-filling of this chamber with the acid. T he crank-case 25 contains an outlet about midway between its top and bottom for the sulphuric acid which connects with a pipe 37 opening into a trap 38 having a valved drain-pipe 39, the opposite end of this trap communicating with a pipe 40 which opens into the drying tower 13.

and terminates above the packing 14*there in, in a spray-head 41 for spraying sulphuric acid against the rising currents of chlorine gas passing upwardly through the tower. .The compressor-outlet pipe 24 containsa'valve 42 and opens into the upper end of a tank 43 of a cooling apparatus 45 the coil of which, for the cooling medium,

and which is located in the tank' 43, being represented at 44. A pipe 46 for cooling water supplied thereto, as hereinafter described, connects with theupper end of the coil 44 for causing "cooling water to flow through the latter from which it discharges through a pipe 47 into the jacketed portion of-the cylinder 48 of the compressor, the outlet of this jacketed portion beingrepresented at 49 and opening into a sewer.

A pipe 51 leading from a supply (not shown) of cooling water connects with the upper end of a coil (not shown) which lies in the bottom of the crank-case 25, the outlet of this coil communicating with a pipe 53 which connects with a condenser hereinafter referred to.

The'lower end of the tank 43 opens into .end with a valved water-inlet pipe 57 which connects with the pipe 53, the upper end of the coil 56 being connected with the pipe 46, the coil 54 and 56 forming a condenser in which the cooling water travels in a direction contrary to the flow of the gas. A pipe' 54 preferably connects with the pipe 54 and has branch pipes 54 and 54, the pipe 54* being equipped with a gauge 54 and the pipe 54? which forms a vent-pipe, being equipped with a valve 54*. A pipe 58 valved at 59 leads from the coil 54 to a T-coupling 60 one outlet of which connects with a pipe 61 connected by a flexible'pipe 61 with a pipe 61 which terminates in a hollow head 62 with a valve 63, this head being connected by 64 with the inlet of a shipping container represented at 65, the container shown being such as are commonly used and holding about 100 pounds of liquid chlorine, the container being enclosed in heat-insulating material represented at 66 and shown as supported on a weighing scale 70. The other outlet of the T-coupling 60 connects with a pipe 67 having an enlargement 68 with a valve 69 below the enlargement, this pipe opening into the upper end of the drying tower 16 and terminating therein in a sprayhead (not shown) for spraying sulphuric acid, separated the chamber 68 from the liquid chlorine, into the chlorine gas as it passes upwardly through this tower.

In the operation of the apparatus as shown, the chlorine gas is drawn from the electrolytic cells hereinbefore referred to, by

a slight vacuum preferably of about A, to A of water, produced b the action of the compressor and regulate by the valve 22, the gas with its contained water-vapor which is present'to a considerable degree and which should be removed, passing throu h the pipe 3 into the coil 4 wherein it is sn jected to the cooling'action of the water flowing into the latter through the pipe 7 and rents of the gas contacting the packing 14 which is wetted by the discharge of acid against it, the acid being supplied through the spray-head 41 from the pipe 40, trap 38,

pipe 37 and .crank-case 25, the acid thus used being the acid which has passed through the compressor crank-case 25 and has overflowed therefrom under the action of the continuous feed of acid into the crankcase-from the tank 30, the acid flowing from the tower 13 through a pipe 13 at its bottom and discharging into a receptacle. 13* below its outlet 13 from which the spent acid flows to storage or waste. The gas then passes from the upper end of the drying tower 13 into the lower end of the drying tower 16 through which latter it upwardly passes in contact with the packing 14 wetted with a sl'ower'of sulphuric acid from the spray-head (not shown) but hereinbefore referred to and supplied with sulphuric acid from any suitable source, supplemented by sulphuric acid which passes into the pipe 67 from the separator-chamber 68, the moisture in the gas being reduced thereby to about 0.3 to 0.5 milligrams per liter, the final drying of the gas taking place in the tower 16. The gas then passes through the coil 18 where it is subjected to the cooling action of expanding chlorine gas which is supplied to the coil 19', to flow in a direction therethrough opposite to the flow of the gas through the coil 18, from the chamber 43 through the pipe 20. The gas in cooled condition then passes through the valved pipe 18 into the inlet of the compressor where it is. compressed to about 100 pounds per square inch and in the compressing o eration is coinmingled with sulphuric aci in finely divided condition and preferably partially vaporized, the acid being fed to the piston for lubricating it by the splash-feed action thereupon the air exhausted from the conand thenceinto the upper end of the tank 43 f the cooling apparatus 45, which operates as a trap, where it is subjected to the cooling action of the water which enters the coil 44 therein from the pipe 46 and discharges through the pipe 47 into the jacket of the compressor to prevent overheating of its cylinder 48. Condensing of a portion of the chlorine and sulphuric acid is efiected in the tank 43, the acid, being heavier than the liquid chlorine, gravitating to the bottom of this tank and flowing with chlorine through the pipe 20 and coil 19 back to the crank case"25. The chlorine either as gas .or liquid passes from the tank 43 through the pipe 54, which preferably is located a considerable distance from the bottom of the tank 43, into the condenser-54 which completes the condensing of the chlorine gaswhich passes over from the cooling tank 43, the chlorine in passing through the condenser-.54 being subjected to the cooling action of the oppositely flowing currents of cold water-in the coil 56. The condensed chlorine and any condensed sulphuric acid content, discharges into the pipe 58, the acid settling in the chamber 68 and theliquid chlorine entering the pipe 61 from which the chlorine, which is'substantially 100% pure, maybe filled into the shipping containers such, for example, as the one shown at 65.

The eifect of operating on the chlorine as described is to produce in the condensing apparatusbeyond the compressor, liquefied chlorine ata temperature of the coil 54 'of approximately F. and under relatively low pressure as stated, thus permitting the liquefied chlorine to be directly charged into the shipping containers. In the filling of the containers the air is exhausted therefrom before the filling operation begins, this exhausting operation being effected in any desired manner. -The container is preferably first cooled to a point below the temperature of the condensed chlorine and then enclosed in the'lhsulating covering 66 and tainer. The container is then connected with the pipe 61. and the liquid chlorine then permitted to flow into the container, this filling operation being quickly etfected. The'insulating o the container 65 serves to keep down the as pressure in the coil 56 and this is further facilitated by permittinga'portion of the liquid chlorine in the container 65 to evaporate by closing the valve 59 and opening val e 69. The gas thus liberated, to-

- gether ,with the accumulations of'acid in chamber 68, flows back through pipe 67 to the tower 16 and is thus not wasted. The temperature of the containers may thus be caused to be less than the temperature of the water in the condenser coil 56 so that no additional gas pressure is required for filling the containers. The feature of exhausting the airfrom the containers also presents the advantage of preventing the passage of air therefrom into the condenser and thereby producing objectionable results.

The efiect of. causing the compressed chlorine gas and-sulphuric. acid to become commingled, is to render the compressed chlorine gas, condensable at such a relatively high temperature that the chlorine gas may.

even though quite impure, and compressed only to the relatively low degree of substantially 1-00 pounds to the'square inch, be condensed at relatively high temperature as for example 70 F the temperature of ordinary water, with the manifest advantages, especially over prior practices involving the, refrigeration of the compressed gas to temperatures at, or .approximatelypat, 35 F. below zero. While I prefer to employ sulphuric acid for the. purpose stated, if desired, other substances condensable at hi her temperatures, than that at which pure. hlorine under the same pressure condenses, maybe used and the commingling of such subsired way, as-also the .commingling of the sulphuric acid and-the gas may be effected in other ways, than that described.

The feature of maintaining a pressure of chlorine gas in the crank-case is of advanpanding chlorine into lofiv-pressure gas in the coil 18 s ofadvantage as it aids in keeping cool the bearings of the compressor and reduces the final pressure requiredin the liquefying coil 54.

The water from waste49 may, if desired,

be used in the preliminary cooler 5 where temperature conditions permit; and the trap 38 is made sufliciently deep to more than counterbalance the gas pressure in the crank-1 case, so that .no chlorine gas can get back into the tower 13.

When the container 65 has been filled the valves 59 and 62 are closed and valve 69 opened for a moment to relieve the. gas in 1 these connections.

The pipe 34, which is preferably equipped with a auge 34 and a valve 34 operates to equa ize the pressure in the top of the chamber 30 to effect free gravity-flow of the acid therefrom.

The pipe 20 is preferably equipped with a- 05- stance and the gas, accomplished in any devalve by means of which the pressure of gas manufacture, Ido'not wish to be understood as limiting it thereto.

What I claim as new, and desire to secure by Letters Patent, is:

1. In, the manufacture of liquefied gas,

the method of condensing and discharging the gas into shipping containers without admixture of the gas with air, which consists in compressing and condensing the gas, removing the air from the containers and in evacuated condition introducing the condensed gas into the containers while maintaining the latter at a temperature lower than the liquefied gas during condensation.

2. In the manufacture of liquefied chlorine gas, the method of condensing and discharging the 'gas into shipping containers without admixture of the gas with air, which consists in compressing and-condensing the gas, removing the air from the containers and in evacuated condition introducing the condensed gas into the containers while maintaining the :latter at a temperature lower than the liquefied gas during condensation.

3. In the manufacture of liquefied gas, the method of condensing and discharging the gas into shipping containers without admixture of the gas with air, which consists in removing the air from the containers, cooling the containers, thereupon introducing the liquefied gas into the containers and permitting it to expand therein by relieving the pressure in the container to produce a cooling'acti'on on the containers and thereafter completing the filling of the containers with the liquefied gas.

' 4.'In the manufacture of liquefied chlorine gas, the method of condensing and discharging the gas into shipping containers without admixture of the gas with air, which consists in removing the air from the containers, cooling the containers, thereupon introducing the liquefied gas into the containers and permitting it to expand therein 'by relieving the pressure in the container to produce a cooling action'on the containers and thereafter completing the filling of. the

containers with the liquefied gas.

1 container and iii e' 5. In apparatus for condensing gas and filling containers therewith, the combination of means for condensing compressed gas, a shipping "receptacle from which the air has been removed, in communication with the discharge of said condensing means, and valve means controlling the discharge'of the liquefied gas-from said condensing means into said receptacle.

- 6. In the manufacture of liquefied gas, the method of condensing and charging the gas into shipping containers without admixture of the gas with air, which consists in first removing the air from the container and in evacuated condition introducing the gas into it, after the condensing thereof, relieving the pressure .in the container to permit volatilization and thereby chill the-container,

and thereafter completing the charging of the container with the condensed as,

7. In the manufacture of lique ed chlorine' gas, the method of condensing and charging the gas-. into shipping containers without admixture'of the gas with air, which consists in firstrerno ing the .air' from the tedj condition introduci'ng the gasinto fter the;,condensing thereof, relieving thepres'surelin the. container to permit volatilization and=-- thereby chill the container, and thereaftercompleting the charging of the container; 'th' the condensed gas.

8. In the manufacture of liquefie' 'gas, the method of condensing anddischarging gas into shipping containers without the admixture of the gas with air, which consists in removing the air from the containers, thereupon introducing the liquefied gas into ,the containers and permitting it to expand therein by relieving the ressure in the container to' produce a coo ing action on the containers and thereafter completing the charging of the containers with the liquefied 9. In the manufacture of liquefied gas, the method of condensing and discharging the gas into shipping containers without admixture of the gas with air, which consists in liquefying the gas, removing the air from the containers and, in evacuated condition, introducing the gas, after condensing it, into the containers, relieving the pressure in the containers to permit volatilization and thereby chill the containers, thereafter oompleting the charging of the containers with the condensed gas, and maintaining the com tainers during the charging at a temperature not exceeding that of the liquefied gas during condensation.

WILLIAM M. JEWELL.

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